CN103196919A - Method for identifying precipitate corrosion pit positioned on surface of tellurium-zinc-cadmium crystal - Google Patents

Method for identifying precipitate corrosion pit positioned on surface of tellurium-zinc-cadmium crystal Download PDF

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Publication number
CN103196919A
CN103196919A CN2013101003036A CN201310100303A CN103196919A CN 103196919 A CN103196919 A CN 103196919A CN 2013101003036 A CN2013101003036 A CN 2013101003036A CN 201310100303 A CN201310100303 A CN 201310100303A CN 103196919 A CN103196919 A CN 103196919A
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China
Prior art keywords
crystal
etch pit
cadmium
tellurium
corrosion
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CN2013101003036A
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盛锋锋
杨建荣
孙士文
周昌鹤
虞慧娴
徐超
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Shanghai Institute of Technical Physics of CAS
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Shanghai Institute of Technical Physics of CAS
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Abstract

The invention discloses a method for identifying precipitate corrosion pits positioned on the surface of a tellurium-zinc-cadmium crystal. The method comprises the following four steps of: crystal surface preprocessing, crystal surface cleaning, corrosive liquid preparation, crystal surface corrosion and crystal defect observation and identification. The method is characterized in that the conventional optical microscope is used for observing the corrosion pit positioned on the surface of the tellurium-zinc-cadmium crystal in the step of crystal defect observation and identification; the bottom surfaces of the corrosion pits are rough in a 1000-magnification view field, thus the black defects corresponding to the corrosion pits which are in triangular shapes, hexagonal shapes or irregular shapes under a microscope are precipitates; isolated corrosion with peripheral materials in pit shapes are the corrosion pits formed by tellurium-rice precipitates pits by being observed in a 50-magnification view field; and the corrosion pits with a large quantity of dislocation corrosion pits congregated in the peripheral materials are the corrosion pits formed by cadmium-rich precipitates. The method disclosed by the invention has the characteristics that various precipitate corrosion pits can be directly identified on the surface of a tellurium-zinc-cadmium material and research and fast detection of the precipitate can be convenient.

Description

A kind of recognition methods of tellurium-zincium-cadmium crystal surface precipitation thing etch pit
Technical field
Patent of the present invention relates to a kind of recognition methods of defects from semiconductor materials etch pit, specifically refers to a kind of recognition methods of tellurium-zincium-cadmium crystal surface precipitation thing etch pit.
Background technology
Tellurium zinc cadmium material is a kind of semiconductor material that is widely used, be mainly used in the backing material of tellurium cadmium mercury epitaxial and absorb gamma-ray material, the infrared focal plane detector and the gamma ray detector that prepare with its have application widely in fields such as spacer remote sensing technology, safety check technology, medical diagnosis technology and weaponrys.Owing to be subjected to the restriction of growing technology, exist micron-sized sediment defective in the tellurium-zincium-cadmium crystal inevitably, sedimentary density is in (1~10) * 10 3Cm -3The sediment defective can directly influence the performances such as responsiveness, noise and blind element rate of gamma ray detector as the carrier capture center, also can traverse in epitaxial process in the tellurium cadmium mercury epitaxial material simultaneously, causes the performance of HgCdTe infrared focal plane device to descend.Therefore, the sediment defective in the tellurium-zincium-cadmium crystal is disclosed, identifies and detects is one of critical process of detector preparation, also is simultaneously that research and improvement tellurium-zincium-cadmium crystal growing technology are necessary.Observing the sedimentary classic method of tellurium-zincium-cadmium crystal carries out at the infrared transmission microscopically, because the resolution of infrared camera is low, add that rich cadmium sediment can change along with the variation of microscope transmitted light intensity at the pattern of infrared transmission microscopically, therefore this method can not accurately be understood the sedimentary appearance structure of rich cadmium.As utilize the sedimentary density of infrared transmission microscopic examination, and shortcoming has three: 1, and enlargement ratio needs at least more than 200 times, and it is very little to observe the visual field accordingly, and the distribution of sediment in crystal is very inhomogeneous, therefore the precipitate density error that obtains is bigger; 2, need material is carried out 3-D scanning to obtain volume density, it is longer to detect the time that needs like this; 3, when making the backing material of tellurium cadmium mercury epitaxial with tellurium zinc cadmium material, relatively paying close attention to is the defect concentration on tellurium-zincium-cadmium crystal surface, is transformed into surface density from the sediment volume density and need measures sedimentary average-size, this not only needs to spend the plenty of time, and also out of true of the result who obtains.The method that overcomes these shortcomings is to disclose defective by corrosion at plane of crystal, observes and detect defect concentration then under conventional optical microscope.There is a problem in this method, namely how to identify the sediment etch pit on tellurium-zincium-cadmium crystal surface, and comes with conventional dislocation etch pit difference.The present invention is directed to this problem, a kind of recognition methods of tellurium-zincium-cadmium crystal surface precipitation thing etch pit is provided.
Summary of the invention
The purpose of this invention is to provide a kind of recognition methods of tellurium-zincium-cadmium crystal surface precipitation thing etch pit, be used for solving the problem that prior art can not be identified the various sediment defectives on tellurium-zincium-cadmium crystal surface.The recognition methods of tellurium-zincium-cadmium crystal surface precipitation thing etch pit comprises that plane of crystal pre-service, plane of crystal clean, prepare corrosive liquid and corrode plane of crystal and observe 4 steps of identification crystal defect, and concrete steps are as follows:
1. get the cadmium zinc telluride crystal wafer that obtains along the cutting of (111) face, (111) B face is removed cutting damage layer and the glossy surface of dishing out with mechanical buffing;
2. cadmium zinc telluride crystal wafer is cleaned 3 times with the triclene that boils, falls behind the triclene with 0.2%Br-methanol solution corrosion 30s~60s with washed with methanol, again with washed with methanol fall from the isopropyl alcohol that boils, take out behind the corrosive liquid stand-by;
3. press red fuming nitric acid (RFNA): hydrofluorite: hydrogen peroxide: the volume ratio preparation corrosive liquid of deionized water=10:10:8:12, cadmium zinc telluride crystal wafer is put into corrosive liquid, at room temperature corrode after 3 minutes and take out, clean up with deionized water, dry up with nitrogen then;
4. use conventional observation by light microscope cadmium zinc telluride crystal wafer (111) B surface, determine the corresponding defective of etch pit according to the characters and appearances of all kinds of defective etch pits, specific practice is as follows: under 1000 multiplying power visual fields, the defective of the triangular planar pit that the etch pit basal surface is level and smooth and triangle conical pit correspondence is the dislocation (see figure 1); Under 1000 multiplying power visual fields, therefore the etch pit basal surface is coarse and to become triangle, hexagon or the corresponding defective of irregular shape etch pit of black at microscopically be sediment, wherein observe under 50 multiplying power visual fields, the isolated etch pit that the material pattern around the etch pit is pit is the etch pit (see figure 2) that rich tellurium sediment forms; The etch pit that has a large amount of dislocation etch pits to gather in the material around the etch pit is the etch pit (see figure 3) that rich cadmium sediment forms.
Of the present inventionly specifically be characterized as: after the corrosive liquid corrosion that cadmium zinc telluride crystal wafer is formed via nitric acid, hydrofluorite and hydrogen peroxide, under conventional optical microscope 1000 multiplying power visual fields, observe, therefore the etch pit basal surface is coarse and to become triangle, hexagon or the corresponding defective of irregular shape etch pit of black at microscopically be sediment, wherein observe under 50 multiplying power visual fields, the isolated etch pit that the material pattern around the etch pit is pit is the etch pit that rich tellurium sediment forms; The etch pit that has a large amount of dislocation etch pits to gather in the material around the etch pit is the etch pit that rich cadmium sediment forms.
Characteristics of the present invention are: directly identified the corresponding etch pit of various sediments on the tellurium-zincium-cadmium crystal surface, because the characters and appearances size of sediment etch pit goes out several times greatly than the size of sediment itself, make the sediment defective that need adopt the visual field more than 200 multiplying powers to observe at the infrared transmission microscopically originally under conventional optical microscope, to observe and to detect with the visual field of 50 multiplying powers, enlarged markedly the visual field area of observing, conveniently in bigger area, detect precipitate density, can improve accuracy of detection, also significantly reduce the required time of detecting simultaneously.
Description of drawings
Fig. 1. the pattern photo of dislocation etch pit under 1000 multiplying powers on tellurium zinc cadmium material (111) B surface, a is the pattern in the flat hole of triangle, b is the pattern in triangular pyramidal hole.
Fig. 2. the pattern photo of rich tellurium sediment etch pit under 50 multiplying powers on tellurium zinc cadmium material (111) B surface provided the pattern of rich tellurium sediment etch pit under 1000 multiplying powers on the angle.
Fig. 3. the pattern photo of rich cadmium sediment etch pit under 50 multiplying powers on tellurium zinc cadmium material (111) B surface provided the pattern of rich cadmium sediment etch pit under 1000 multiplying powers on the angle.
Fig. 4 using method process flow diagram of the present invention.
Embodiment
The concrete processing step that adopts of the inventive method is as follows:
1. get the cadmium zinc telluride crystal wafer that obtains along the cutting of (111) face, (111) B face is removed cutting damage layer and the glossy surface of dishing out with mechanical buffing;
2. cadmium zinc telluride crystal wafer is cleaned 3 times with the triclene that boils, falls behind the triclene with 0.2%Br-methanol solution corrosion 30s~60s with washed with methanol, again with washed with methanol fall from the isopropyl alcohol that boils, take out behind the corrosive liquid stand-by;
3. press red fuming nitric acid (RFNA): hydrofluorite: hydrogen peroxide: the volume ratio preparation corrosive liquid of deionized water=10:10:8:12, cadmium zinc telluride crystal wafer is put into corrosive liquid, at room temperature corrode after 3 minutes and take out, clean up with deionized water, dry up with nitrogen then;
4. use conventional observation by light microscope cadmium zinc telluride crystal wafer (111) B surface, determine the corresponding defective of etch pit according to the characters and appearances of all kinds of defective etch pits, specific practice is as follows: under 1000 multiplying power visual fields, the defective of the triangular planar pit that the etch pit basal surface is level and smooth and triangle conical pit correspondence is the dislocation (see figure 1); Under 1000 multiplying power visual fields, therefore the etch pit basal surface is coarse and to become triangle, hexagon or the corresponding defective of irregular shape etch pit of black at microscopically be sediment, wherein observe under 50 multiplying power visual fields, the isolated etch pit that the material pattern around the etch pit is pit is the etch pit (see figure 2) that rich tellurium sediment forms; The etch pit that has a large amount of dislocation etch pits to gather in the material around the etch pit is the etch pit (see figure 3) that rich cadmium sediment forms.

Claims (1)

1. the recognition methods of a tellurium-zincium-cadmium crystal surface precipitation thing etch pit, comprise the plane of crystal pre-service, plane of crystal cleans, the preparation corrosive liquid also corrodes plane of crystal and observes 4 steps of identification crystal defect, it is characterized in that: in the step of observing the identification crystal defect, use conventional optical microscope that the etch pit on cadmium zinc telluride crystal wafer surface is observed, under microscope 1000 multiplying power visual fields, therefore the etch pit basal surface is coarse and become the triangle of black at microscopically, hexagon or the corresponding defective of irregular shape etch pit are sediment, wherein observe under 50 multiplying power visual fields, the isolated etch pit that the material pattern around the etch pit is pit is the etch pit that rich tellurium sediment forms; The etch pit that has a large amount of dislocation etch pits to gather in the material around the etch pit is the etch pit that rich cadmium sediment forms.
CN2013101003036A 2013-03-26 2013-03-26 Method for identifying precipitate corrosion pit positioned on surface of tellurium-zinc-cadmium crystal Pending CN103196919A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104532172A (en) * 2014-12-09 2015-04-22 中国科学院上海技术物理研究所 Heat treatment method for eliminating tellurium-rich precipitate-phase defect in tellurium-zinc-cadmium material through two-step process
CN107192660A (en) * 2017-05-27 2017-09-22 中国科学院上海技术物理研究所 It is a kind of to be used for the apparatus and method that dynamic observes Cdl-x_Znx_Te chemical attack hole
CN109738469A (en) * 2018-12-29 2019-05-10 赛纳生物科技(北京)有限公司 A kind of compactness detection method of FOP surface micro-pit plated film
CN117871218A (en) * 2024-03-13 2024-04-12 南昌航空大学 Subregion division and microstructure display method of ferrite heat-resistant steel heat affected zone

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WO1999059199A1 (en) * 1998-05-11 1999-11-18 Japan Energy Corporation CdTe CRYSTAL OR CdZnTe CRYSTAL AND METHOD FOR PREPARING THE SAME
CN101907576A (en) * 2010-06-11 2010-12-08 中国科学院上海技术物理研究所 Method for testing spatial extension characteristic of tellurium-zinc-cadmium material defect
CN102507584A (en) * 2011-11-10 2012-06-20 中国科学院上海技术物理研究所 Method for detecting sediment area density of tellurium-zinc-cadmium crystal

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WO1999059199A1 (en) * 1998-05-11 1999-11-18 Japan Energy Corporation CdTe CRYSTAL OR CdZnTe CRYSTAL AND METHOD FOR PREPARING THE SAME
CN101907576A (en) * 2010-06-11 2010-12-08 中国科学院上海技术物理研究所 Method for testing spatial extension characteristic of tellurium-zinc-cadmium material defect
CN102507584A (en) * 2011-11-10 2012-06-20 中国科学院上海技术物理研究所 Method for detecting sediment area density of tellurium-zinc-cadmium crystal

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104532172A (en) * 2014-12-09 2015-04-22 中国科学院上海技术物理研究所 Heat treatment method for eliminating tellurium-rich precipitate-phase defect in tellurium-zinc-cadmium material through two-step process
CN107192660A (en) * 2017-05-27 2017-09-22 中国科学院上海技术物理研究所 It is a kind of to be used for the apparatus and method that dynamic observes Cdl-x_Znx_Te chemical attack hole
CN107192660B (en) * 2017-05-27 2023-09-12 中国科学院上海技术物理研究所 Device and method for dynamically observing tellurium-zinc-cadmium material chemical corrosion pits
CN109738469A (en) * 2018-12-29 2019-05-10 赛纳生物科技(北京)有限公司 A kind of compactness detection method of FOP surface micro-pit plated film
CN117871218A (en) * 2024-03-13 2024-04-12 南昌航空大学 Subregion division and microstructure display method of ferrite heat-resistant steel heat affected zone
CN117871218B (en) * 2024-03-13 2024-05-31 南昌航空大学 Subregion division and microstructure display method of ferrite heat-resistant steel heat affected zone

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Application publication date: 20130710